Method of conditioning a hard soap for solvent extraction



Feb 3 E949 J. M. TABoR ET Al.-

v METHOD OF CONDITIONING A HARD SOAP FOR lSOLVENT EXTRACTION :s sheets-snee; 1

Filed Aug. 1, 1945 Peb. s, 1949.`

J. M. TABOR ET AL METHOD OF CONDITIONING A HARD SOAP FOR SOLVENT EXTRACTION 5 Sheets-Sheet 2 Filed Aug. 1, 1945 Mb AILwE ww Feb. 8, 1949. J. M TABOR ET AL '2,461,300

'METHOD OF CONDITIONING A HARD SOAP FOR SOLVENT EXTRACTION` www Patented Feb. 8, 1949 UNITED STATES PATE Nr oF'FlcE METHOD or CONDITIONING A HARD s'oAP` FOR soLvEN'r EXTItAc'IIoN y John Ivi. Tabor, East slip, N; Y., Howard .F. Y Seibert, Mason, Mich., and Paul R. Frohring, Bainbridge, Ohio, assignors to General Biochemicals, Inc., Chagrin Falls, Ohio, a corpora tion of Ohio Original application October 13, 1943, Serial No. 506,060. Divided and this application August 1, 1945, Serial No. 608,280 f 1 Claim. l This invention relates to method and apparatus for extracting pigments, including specically carotene, and oarotin'oid pigments, from fatty materials, such, for example, as animal or vegetable oils and fats.

in object of the invention is to provide a simple and efficient method and apparatus for extracting pigments including plant pigments.

Another Vobject of ,the invention is to provide lmethod and ,means by which soap lumps formed in the extraction ofpigment are powdered and pigment entrapped therein is freed and recovered.

A Another object` is to provide practical, commercial apparatus comprising a closed fluid system.

Another object of the invention is to provide apparatus comprising a single vessel in which all step. j

Other objects will be in part obvious or in part pointed out hereinafter.

TheV invention accordingly consists in the fea-ftures of construction, combinations of elements, arrangements of parts, and in the several steps `and relation and order of each of said steps to one or more of the others thereof, all as will be pointed out in the following description, and the,.

scope of the application of which will be indicated in the following claim.

TheV invention will best be understood if the following description is read in connection with the drawings, in which,

Figure` 1 is a front elevation showing diagrammatically apparatus for carrying out the inven- Figure 2 is an elevational view, partly in secsection being taken on the line 2 2 of Figure 3; Figure 3 is a plan View oi the apparatus; and

- Figure Li is an end View looking, in the direction of the arrow shown in ,Figure 2 and marked Fig sel I0, to the dump doors, d, provided in the wall vof vessel likte dischargethe solid material when these doors are opened, as for example for remov- Ving soap formed' in the vessel by extracting steps 4, with the end casing largely broken Vaway to a vacuum pump, with a solvent tank, and with an extract tank, if desired, sor that all the steps of a pigment extraction operation may beperformed in said ves/sel, and saidvessel and the containers tion, of apparatus embodying the invention, the 40' to which it is connected mly comprise a closed system.`

Vessel l0 is stationary and extending through Vit is a rotatable shaft 65 which is reduced in diameter at its ends which are journalled in bearings 6 5 supported 4en the upright support members 61, Between theends of vessel I i) and the bearings 66 respectively the shaft 65 is provided with and extends through, the stuffing boxes 65% Fixedly mounted on shaft 65 are a number of spiral paddle and scraper members 68 secured at their ends tothe arms projecting radially from collars l0 secured on shaft 55. It will be noted that shaft is somewhat eccentric with respect to vessel l0 so that the spiral paddle and scrapermembersin revolving therein With shaft 65 will lcome very vclose to the inside of the peripheral wall of vessel AHl at the bottom of the vessel, and will have more clearance at the top of the vessel. The members 68 serve both to agitate the fluid contents of vessel I0, and to scrape and ad- Vance solid material, formed or collected, in vesperformed therein, and, il it Ais desirable their direction of rotation may be reversed at times to direct material'fromthe extreme ends of vessel l0 toward the dump doors, d.

A port p is provided extending through an end wall of vessel l0, preferably just inwardly of the circumferential wall to give access to the interior ofvessel' l0 and permit a tool to be inserted into the interior of vesselr l0, as for example to scrape the inner wall of vessel I0 in cleaning it.

The materials which are to be employed, in vessel I0, for an extracting step for example, may be introduced into vessel i0, preferably by way of towers, 'l Iv and 1'2,Y spaced apart longitudinally of vessel l0, through various conduits, and controlled by valvel means, to be described. Shaft 65 may be driven by any suitable source of power (not shown) to rotate the members 69 within vessel |0 to agitate the material within the vessel.

The covers, c, of towers 1I and 12 are provided at the top with windows, w, through which the operator may observe the inside of vessel HJ, and, for example, watch a reaction taking place therein whilethe apparatus is in use so that he may better control it. Thus for example, he may desirev to momentarily release a vacuum, .drawn on the vessel for reasonsto be describectif heobserves foaming.

A closed system of which vessel llly forms the Y ywith the amount of palm oil being treated.

lumps which continues until the soap is in the i form of granules which may be on the order of 100 mesh. The temperature in vessel I0 at atmospheric pressure is raised, by the aforesaid `preheating and by the heat of reaction to a ication step, at a pressure sufficiently less than atmospheric pressure to insure the maintainance of a boiling temperature less than 80 C, For example successful results have been obtained using a vacuum of about twenty-five inches (roughly a pressure of 125 millimeters of mercury), but in any event the pressure should not Vbe allowed to exceed 355 millimeters of mercury,

under which pressure water boils at 80 C. .In the process of treating palm oil or other fatty material which will give a hard soap the pressure varies due to the interaction of alkali with glycerides and therefore cannot be stated in deiinite terms.

The employment of reduced pressures has the further advantages that it results in the exclusion from vessel Ill of air the presence of which-would be detrimental since it would promote decomposition by oxidation of the carotene or other pigment being extracted, and facilitates the breaking down of newly formed soap lumps and the consequent freeing therefrom, and the recovery of, pigment containing material, as well as of free alkali and oil which may become entrapped in the soap lumps. l

Depending upon the characteristics of the particular kind of material or oil to be treated w'e have found, as stated above, that it is some times desirable to employ somewhat more of thealkali solution than is required to provide an amount which is the exact chemical equivalent of the amount of the oil r other fatty material being treated. We have found that certain oils have a tendency to form a soft soap, and thata harder soap, and one having better powdering characteristics, may be obtained by using an amount of alkali solution which is greater than the chemical equivalent of the particular oil or other fatty material being treated, the increased amount, over and above the chemical equivalent amount, being determinable by experimentation in each case. Thus, for example, we have found that in the treatment of palm oil we obtain very satisfactory results employing twenty percent more of the aforesaid fifty percent aqueous caustic alkali than is necessary for chemical equivalency In the operation vof the apparatus set forth herein the `vessel I0 -may be initially heated, as by filling steam jacket 16 with steam to preheat the oil which is first drawn into vessel I ll,.but the supply of steam to the steam jacket is preferably throughout the oil because, if even distribution is not' obtained,'heavy balls of soap may, form which in addition to being slow anddicult to break up, may impede and interfere with the rotation of members B8. As stated above, we provide one or more windows win the covers c of the towers or domes 'Il and 12 of vessel l vthrough which the operator may watch the reaction closely, and if he observes any tendency of the mixture to foam he should release the vacuum momentarily, as by opening vacuum release valve Il)b which communicates with the interior of vessel lll through line Illa.

During the saponiflcation step the heat in vessel I resulting from the reaction of the oil and alkali, and increased by the preheating 'step which is preferably employed, is suiiicient to ash off the water in which the alkali was dissolved and the reduced pressure employed facilitates the flashing oi of the water including that which is progressively released from the soap lumps as they divide and disintegrate into smaller lumps. The water vapor is withdrawn through vapor line 24, dust trap 23, and line 22, into condenser 2l where it is condensed, and may be drawn'off, through an outlet, not shown, and discarded, when the saponication step is completed. The

soap, at the end of the saponificationstep'is in a very dry and finely powdered condition which requires no further processing before Vthe pig-v ment is extracted.

. agitation is recommenced and continued for approximately fifteen minutes or until the soap is thoroughly wetted. When the solvent and soap have been intimately mixed, agitation is discontinued ard the soap'and theV extract bearing solvent are allowed to separate 'by gravity. When a solvent is used which has a specific gravity greater than soap the clear extract bearing solvent is drawn off into the extract storagey tank 3| through conduits 32 and. 31, and pump, as described above. When the solvent employed has a specific gravity less than the soap, taps will vbe provided to draw the solvent from the top of the vessel. Y Y

When the extract bearing solvent being 'withdrawn becomes cloudy as seen through line sight s in line 32, the withdrawal should be stopped. When all the clear extract bearing solvent has been drawn out of vessel I0, fresh solventV for another wash may be ldrawn into vessel I0, in the manner set forth above, and agitation isresumed for approximately fifteen minutes or until the remaining soap is again thoroughly wetted q with solvent, after which the agitation is stopped,

-the soap and the extract bearing solventV are again allowed to separate, and, after separation, the extract bearing solvent is drawn off again, as describedabove.

The extracting step may be repeated in this way as many times as economy of time and material permit. j

After the additional washing steps, which com.-

solvent extraction, which soap is formed by aqueous-alkaline saponication of a, fatty oil containing unsaponifiable oil-soluble pigment material, the improved step which comprises: mixing fatty oil and an excess of aqueous alkaliunder vacuum in a closed saponioation zone, continuously agitating the saponiflcation mixture,` continuously maintaining a pressure in the saponication zone not exceeding 355 mm. of mercury throughout the saponification by continuously exhausting gases and vapors therefrom, and continuing said agitation and the maintenance of said sub-atmospheric pressure until the soap formed is substantially dry, whereby the heat of saponication is utilized to boil 01T water entrappedin soap lumps Vformed during saponification 'at-:temperature substantially below the normal boiling point of water and the lumps are thus disrupted and comminuted and the soap is made aceessible to the solvent.

JOSEPH M. TABOR. HOWARD F: SEIBERT. PAUL R. FROHRING.

10 mimEmcsrmisy CITED The following references are of record in the file of this patent: -V

y UNITED STATES PATENTS Number Name Date 1,338,698 Richardson May 4, 1920 1,807,232 Wurst'er et al May 26, 1931 1,813,575 Janecke et al July 7, 1931 1,919,229 Lovett 1;; July 25, 1933 2,031,991 Ung'nade et al ilf'eb. 25, 1936 2,179,872 Peebles Aug. 29, 1939 2,325,195 Carlson et al ;*July 13, 1943 2,265,830 Taylor Dec. 23, 1941 22715406 Thurman Jan. 17, 1942 2,313,747 Buxton .-May 11, 1943 23133748 Buxton May 11, 1943 2,383,631

Trent `Aug. 28, 1945 

